TW201634747A - 銀被覆粒子及其製造方法 - Google Patents
銀被覆粒子及其製造方法 Download PDFInfo
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- TW201634747A TW201634747A TW105102227A TW105102227A TW201634747A TW 201634747 A TW201634747 A TW 201634747A TW 105102227 A TW105102227 A TW 105102227A TW 105102227 A TW105102227 A TW 105102227A TW 201634747 A TW201634747 A TW 201634747A
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Abstract
本發明係提供備有,由無機或樹脂粒子所形成之芯粒子(2),與形成於該芯粒子(2)之表面上之銀被覆層(1)的銀被覆粒子(P1),其中銀被覆層(1)中之銀量相對於銀被覆粒子100質量份為5~90質量份,將前述銀被覆粒子(P1)填入X線衍射裝置所附屬之試料托盤中以2 θ/θ=30~120deg之範圍照射X線,再由所得之衍射線算出的銀之結晶粒徑為35~200nm之範圍。
Description
本發明係有關適用為導電性接著劑、導電性薄膜、導電性調距物所含有之導電性填料的銀被覆粒子及其製造方法。更詳細為,係有關製作導電性接著劑等,而將剪斷應力施加於芯粒子與黏合劑樹脂之混合物時銀被覆層不易發生龜裂或斷裂或由芯粒子剝離銀被覆層,可進一步提升導電性接著劑等之導電性的銀被覆粒子。
本申請書係基於2015年1月28日所申請之特願2015-013984號,及2015年12月15日所申請之特願2015-244052號主張優先權,且援用其內容。
有關鉛焊劑之各種替代材料曾檢討導電性接著劑。導電性接著劑為混合樹脂與金屬之導電性粒子之物,代表性之物如導電性糊料及導電性油墨。導電性糊料及導電性油墨因具有優良的應力吸收、低溫安裝、微小間距之導電、絕緣及未使用塑料等之作業性,而被使用於液晶顯示器、觸控面板基板、鍵盤等之電極接續用。為了更
易使用該類導電性糊料及導電性油墨,曾開發樹脂粒子之芯粒子被覆金屬所得的金屬被覆樹脂粒子作為導電性粒子用。該類金屬被覆樹脂粒子具有降低製造成本及重量之優點。曾揭示之金屬被覆樹脂粒子如,將鎳無電解電鍍於樹脂粒子之芯粒子後,於其上方被覆金所得之導電性無電解電鍍粉體(例如參考專利文獻1)。該導電性無電解電鍍粉體為,芯粒子之樹脂粒子強固密合電鍍層之Ni或Ni-Au被膜,故可賦予較高之導電性能性。另外曾揭示,具備球狀樹脂之芯粒子與設置於該芯粒子之表面上之錫吸附層,與被覆於該錫吸附層之表面上之銀,且相對於銀被覆球狀樹脂100質量份之前述銀量為5~80質量份,藉由X線衍射法測定之前述銀之結晶粒徑為18~24nm之範圍的銀被覆球狀樹脂(例如參考專利文獻2)。該銀被覆球狀樹脂為,以錫對球狀樹脂之芯粒子進行觸媒化處理,其次實施銀之無電解電鍍,以提高銀被膜之密合性。
專利文獻1:日本國特開平08-311655號公報(A)(請求項1,段落[0015]、[0016])
專利文獻2:WO 2012/023566(A)(請求項1)
專利文獻1之方法中,樹脂粒子之芯粒子形成Ni-Au複層被膜時,係將鎳無電解電鍍於樹脂粒子之芯粒子後實施金之無電解電鍍以提升樹脂粒子之芯粒子與金之密合性。但該方法需各自進行鎳電鍍、金電鍍之煩雜的電鍍處理,且需要所必須之材料、基材及時間。又,專利文獻2之方法為,以錫進行前處理於球狀樹脂之芯粒子之表面設置錫吸附層後,實施銀之無電解電鍍,將結晶粒徑控制於18~24nm之較小值而使銀被膜細緻化,以提高密合性。但該專利文獻2之方法所得之被覆球狀樹脂中,因其結晶粒徑較小,故被膜之強度不足。此時例如為了製作導電性接著劑,而將高剪斷力施加於被覆銀之球狀樹脂之芯粒子與黏合劑樹脂的混合物時,會因粒界破壞而使銀之被覆層發生龜裂及斷裂,因而發生由芯粒子剝離銀被覆層,恐降低導電性接著劑之導電性。又,其為各向異性之導電性接著劑時,剝離之電鍍片會成為異物恐入侵原本絕緣之間隙而引起錯誤動作。
本發明之目的為,提供製作導電性接著劑等時,將剪斷應力施加於被覆銀之芯粒子與黏合劑樹脂之混合物時,不易因粒界破壞而使銀被覆層發生龜裂或斷裂或由芯粒子剝離銀被覆層,故可進一步提升導電性接著劑等之導電性的銀被覆粒子及其製造方法。
本發明之第一態樣為,備有由樹脂粒子或無
機粒子所形成之芯粒子,與形成於該芯粒子之表面上之銀被覆層的銀被覆粒子中,該銀被覆層所含有之銀量相對於銀被覆粒子100質量份為5~90質量份,將前述銀被覆粒子填入X線衍射裝置所附屬之試料托盤內以2 θ/θ=30~120deg之範圍照射X線,再由所得之衍射線算出的前述銀之結晶粒徑為35~200nm之範圍的銀被覆粒子。
本發明之第一態樣之銀被覆粒子中,藉由一定之X線衍射法測定之結晶粒徑為較大之35~200nm,故藉由銀被覆層相對於芯粒子可具有優良被覆性、密合性及被膜強度。結果使用該銀被覆粒子製作導電性接著劑等時,既使將高剪斷應力施加於被覆銀之芯粒子與黏合樹脂之混合物,也不易因粒界破壞而使銀被覆層發生龜裂或斷裂或由芯粒子剝離銀被覆層,故可進一步提升導電性接著劑等之導電性。
本發明之第二態樣為,包含將由樹脂粒子或無機粒子所形成之芯粒子加入錫化合物之水溶液內,使前述芯粒子之表面形成錫吸附層之步驟,與使用還原劑使形成於前述芯粒子之表面上的錫吸附層進行無電解銀電鍍,製作前述芯粒子之表面具有銀被覆層的銀被覆粒子先驅物之步驟,與水洗前述銀被覆粒子先驅物後乾燥,再以大氣中100℃以上未達250℃之溫度或水洗後立刻以水中100℃以上未達250℃之溫度熱處理0.5~10小時而燒結構成前述銀被覆層之銀結晶粒,使藉由X線衍射法測定之前述銀結晶粒徑為35~200nm之範圍的步驟的銀被覆粒子之製造
方法。
本發明之第二態樣的銀被覆粒子之製造方法中,製作銀被覆粒子先驅物再水洗、乾燥後,係藉由大氣中100℃以上未達250℃之溫度或水洗後立刻以水中100℃以上未達250℃之溫度熱處理0.5~10小時,以燒結銀被覆層內之結晶粒。藉此增加銀之結晶粒徑以提高該結晶粒之結晶化度,使藉由X線衍射法測定之結晶粒徑範圍為35~200nm。結果因熱處理可使銀被覆層更均勻被覆於芯粒子上,且可藉由芯粒子而確實密合,故可得進一步提升導電性之銀被覆粒子。
本發明之第三態樣為,依據第一態樣藉由銀被覆粒子混合黏合劑樹脂而製造導電性接著劑之方法。
以依據本發明之第三態樣之方法製造的導電性接著劑具有優良之導電性。
本發明之第四態樣為,藉由將依據第一態樣混合銀被覆粒子與黏合劑樹脂所得之樹脂組成物塗佈於支撐薄膜表面上以製造導電性薄膜之方法。
以依據本發明之第四態樣之方法製造的導電性薄膜具有優良導電性。
本發明之第五態樣為,藉由將依據第一態樣混合銀被覆粒子與黏合劑樹脂所得之樹脂組成物塗佈於2枚基板中任何一方或雙方之表面後貼合前述2枚基板,以製造導電性調距物之方法。
以依據本發明之第五態樣之方法製造之導電
性調距物具有優良導電性。
本發明可提供,為了製作導電性接著劑等而將剪斷應力施加於芯粒子與黏合劑樹脂之混合物時,不易使銀被覆層發生龜裂或斷裂或由芯粒子剝離銀被覆層,可進一步提升導電性接著劑等之導電性的銀被覆球狀樹脂及其製造方法。
P1‧‧‧銀被覆粒子
1‧‧‧銀被覆層
2‧‧‧芯粒子(母粒子)
3‧‧‧固定用樹脂
P2‧‧‧銀被覆粒子(比較例)
11‧‧‧銀被覆層(比較例)
12‧‧‧芯粒子(母粒子,比較例)
13‧‧‧固定用樹脂(比較例)
圖1為,表示實施例2之銀被覆粒子P1的銀被覆層剖面之TEM像(倍率50萬倍)之圖。又,表示本發明之銀被覆粒子P1之芯粒子2與銀被覆層1,以及固定用樹脂3。
圖2為,表示比較例2之銀被覆粒子P2的銀被覆層剖面之TEM像(倍率50萬倍)之圖。又,表示比較例之銀被覆粒子P2之芯粒子12與銀被覆層11,以及固定用樹脂13。
其次將說明實施本發明之形態。
本實施形態之銀被覆粒子P1為,備有芯粒子2(母粒子),與形成於該芯粒子2之表面上之銀被覆層1。該銀被覆層1所含有之銀量相對於銀被覆粒子100質量份為5~90質量份,且將前述銀被覆粒子P1填入X線衍射裝置所附屬之試料托盤內以2 θ/θ=30~120deg之範圍照射X線,再由所得之衍射線算出銀之結晶粒徑為35~200nm之範圍,較佳為40~80nm之範圍,銀被覆層1係以無間隙狀被覆於芯粒子2。銀之結晶粒徑未達35nm時銀被覆層1無法以無間隙狀被覆於芯粒子2,而使相對於芯粒子2之銀被覆層1之被覆性、密合性與被膜強度較差。超過200nm時會因製造過程之燒結而使銀被覆層1收縮,使銀凝聚於芯粒子2上方,故易降低銀被覆層1之被覆率,又,芯粒子2為樹脂粒子時會變形而損害銀被覆粒子P1之外觀,且恐剝離銀被覆層1。
本實施形態之銀被覆粒子之製造方法為,包含將上述芯粒子2加入保溫為25~45℃之錫化合物之水溶液內使上述芯粒子2之表面形成錫吸附層之步驟,與使用還原劑使形成於上述芯粒子2之表面上之錫吸附層進行無電解銀電鍍而使芯粒子2之表面具有銀被覆層1以製作銀被覆粒子先驅物之步驟,與水洗上述銀被覆粒子先驅物後乾燥再以大氣中100℃以上未達250℃之溫度或水洗後立刻以水中100℃以上未達250℃之溫度進行0.5~10小時熱處理之步
驟的方法。
銀被覆粒子P1之母體的芯粒子2係包含形狀上圓形度較高之球狀粒子或圓形度較低之異形粒子。球狀粒子可為實質上球狀之狀子,例如包含完整球形之粒子、橢圓形般近似球形形狀之粒子、表面具有若干凹凸粒子。異形粒子如棒狀、板狀、鱗片狀之粒子。又,芯粒子2係由材質為樹脂粒子或無機粒子所形成。
樹脂之芯粒子2如聚矽氧系、丙烯酸系、苯酚系或苯乙烯系樹脂。因該等樹脂具有較高的銀被覆粒子P1使用於各向異性之導電性接著劑或導電性薄膜等時所要求之特性,例如將荷重施加於填料時填料之破壞性,及去除荷重時之回復率。聚矽氧系樹脂如,聚矽氧樹脂、聚矽氧橡膠、聚矽氧樹脂被覆聚矽氧橡膠等。丙烯酸系之樹脂如,甲基丙烯酸甲酯樹脂(PMMA樹脂)、丙烯酸-苯乙烯共聚合樹脂(AS樹脂)、改質丙烯酸樹脂等,苯酚系樹脂如,苯酚樹脂、苯酚-甲醛樹脂、苯酚-糠醛樹脂等,苯乙烯系樹脂如,聚苯乙烯樹脂、苯乙烯-丙烯腈共聚物、丙烯腈-丁二烯-苯乙烯共聚物樹脂(ABS樹脂)等。無機芯粒子2如,滑石、二氧化矽、雲母、氧化鋁或氮化硼。
芯粒子2之平均粒徑較佳為0.5~40μm之範圍內。芯粒子2之平均粒徑未達0.5μm時會因芯粒子2之表面積較大,而為了得到作為導電性填料或導電性粒子用所
必須之導電性需增加銀量。芯粒子2之平均粒徑大於40μm時銀被覆粒子P1難適用於微細圖型中。
芯粒子2之平均粒徑係使用日立高科技股份公司製掃描型電子顯微鏡(型號:S-4300SE),藉由軟體(品名:PC SEM)以倍率:2000倍測定300個芯粒子2之粒徑,再算出該測定值之平均值而得平均粒徑。又,具有真球狀以外之形狀的芯粒子2係以長邊平均值作為平均粒徑。
芯粒子2之表面設有銀被覆層1。一般於有機質材料或無機質材料等不導體之表面實施無電解電鍍時,需預先對不導體之表面進行觸媒化處理。本實施形態中係以芯粒子2之表面上進行錫吸附層設置處理以作為觸媒化處理用,其後進行無電解銀電鍍處理以形成銀被覆層1。具體上本實施形態之銀被覆層1為,藉由將芯粒子2加入保溫為25~45℃之錫化合物之水溶液內於該芯粒子2之表面形成錫吸附層後,使用還原劑使該錫吸附層進行無電解銀電鍍,而形成於芯粒子2之表面。本說明書中將藉由無電銀電鍍而於芯粒子2之表面形成銀被覆層1之物稱為銀被覆粒子先驅物,將該先驅物熱處理後所得之物稱為銀被覆粒子P1。
為了形成上述錫吸附層,將芯粒子2加入錫
化合物之水溶液後進行攪拌,再濾取芯粒子2進行水洗。攪拌時間係由下述錫化合物之水溶液之溫度及錫化合物之含量而適當決定,但較佳為0.5~24小時。錫化合物之水溶液之溫度較佳為25~45℃。錫化合物之水溶液之溫度未達25℃時,會因溫度過低而降低水溶液之活性,故錫化合物無法充分附著於芯粒子2。又,錫化合物之水溶液之溫度超過45℃時,會使錫化合物氧化而使水溶液不安定,故錫化合物無法充分附著於芯粒子2。以25~45℃之水溶液實施該處理時,錫之二價離子會附著於芯粒子2之表面而形成錫吸附層。
上述錫化合物如,氯化亞錫、氟化亞錫、溴化亞錫、碘化亞錫等。使用上述錫化合物時水溶液中之錫含量較佳為20g/dm3以上,水溶液可含有至飽和濃度之量。又,為了提升錫化合物之溶解性,相對於水溶液中之錫1g較佳為含有鹽酸0.8cm3以上。
芯粒子2之表面形成錫吸附層後,使用還原劑使該錫吸附層進行無電解銀電鍍而於芯粒子2之表面形成銀被覆層1得銀被覆粒子先驅物。無電解銀電鍍法如,(I)將表面形成錫吸附層之芯粒子2浸漬於含有錯化劑、還原劑等之水溶液中,再滴入銀鹽水溶液之方法,(II)將表面形成錫吸附層之芯粒子2浸漬於含有銀鹽、錯化劑之水溶液中,再滴入還原劑水溶液之方法,(III)將表面形成錫吸附層之芯粒子2浸漬於含有銀鹽、錯化劑、還原劑等之水溶液中,再滴入苛性鹼水溶液之方法。
銀鹽可使用硝酸銀或銀溶解於硝酸之物等。錯化劑可使用氨、伸乙基二胺四乙酸、伸乙基二胺四乙酸四鈉、硝基三乙酸、三伸乙基四胺六乙酸、硫基硫酸鈉、琥珀酸鹽、琥珀酸醯亞胺、檸檬酸或碘化物鹽等之鹽類。還原劑可使用甲醛水、葡萄糖、咪唑、羅謝系鹽(酒石酸鈉鉀)、肼及其衍生物、氫醌、L-抗壞血酸或甲酸等。還原劑就還原力之強度較佳為甲醛,更佳為至少二種以上含有甲醛之還原劑之混合物,最佳為含有甲醛與葡萄糖之還原劑之混合物。
無電解銀電鍍處理過程中,最初係進行錫吸附層之錫與銀離子之取代反應,而於芯粒子2之表面析出形成核之金屬銀。藉由上述取代反應與自己觸媒性還原反應,可於芯粒子2之表面形成具有一定結晶粒徑之銀之被覆層,得銀被覆粒子先驅物。
水洗所得之銀被覆粒子先驅物後乾燥再以大氣中100℃以上未達250℃之溫度或水洗後立刻以水中100℃以上未達250℃之溫度熱處理0.5~10小時,製作銀被覆粒子P1。具體上水洗為,重覆於離子交換水中傾析銀被覆粒子先驅物,並去除上層澄清水使電傳導度至10μS/cm以下為止。又乾燥為,將水洗後之銀被覆粒子先驅物放入不銹鋼瓶般容器內,使用真空乾燥機於維持為50~80℃之溫度下進行。大氣中進行熱處理時係以,將乾燥後之銀被覆粒子
先驅物放入與乾燥時相同之容器內使容積厚為1cm以下,送風乾燥機或電氣馬弗爐中以大氣中保持100℃以上未達250℃之溫度0.5~10小時之方式進行。水中進行熱處理時係以,使乾燥前之銀被覆粒子先驅物為1~20質量%般懸浮於離子交換水後,於高壓釜中以100~300rpm之回轉速度攪拌該懸浮液的同時,保持100℃以上未達250℃之溫度0.5~10小時,較佳為保持後使用真空乾燥機以50~80℃之溫度乾燥過濾懸浮液所得之塊物的方式進行。大氣中進行處理時具有無需特殊設備可簡便處理之優點,水中進行處理時具有可均勻熱處理之優點。其他雖需具有設備,但可使用氣流式乾燥機或噴霧乾燥器之裝置於大氣中進行熱處理。藉由該熱處理可燒結銀被覆層1之銀結晶粒。藉此可增加銀之結晶粒徑而提高其結晶化度。
熱處理溫度未達100℃及熱處理時間未達0.5小時時,銀被覆層1之銀將無法熱擴散而幾乎無法燒結,故結晶化度較低。又,熱處理溫度超過250℃以上及熱處理時間超過10小時時,會因銀被覆層1與芯粒子間之熱應力而發生銀被覆層1剝離,及伴隨著剝離而凝聚銀故不宜。較佳之熱處理溫度為120~200℃,熱處理時間為1~5小時。藉由將該熱處理溫度及/或時間變更為上述範圍內,可控制銀被覆層1之銀之結晶粒徑為35~200nm之範圍內。具體為,提高熱處理溫度或拉長熱處理時間時,燒結銀被覆層1之銀可增加銀之結晶粒徑,又,降低熱處理溫度或縮短熱處理時間時,將無法燒結銀被覆層1之銀,
故銀之結晶粒徑較小。
形成於銀被覆粒子P1之表面上之銀被覆層1所含有的銀量,相對於銀被覆粒子100質量份為5~90質量。銀之被覆量(含量)係由樹脂之平均粒徑所必備之導電性而決定。相對於銀被覆粒子100質量份之銀含量未達5質量份時,既使進行上述熱處理也無法使銀被覆層1無間隙般被覆於芯粒子2,故分散後作為導電性填料或導電性粒子用之銀被覆粒子P1時,將難取得銀相互間之接點而無法賦予充分之導電性。又,銀含量超過90質量份時會增加比重及提高成本,同時會使導電性飽和。該銀含量較佳為28~80質量份,更佳為28~70質量份。
本實施形態之銀被覆粒子P1作為導電性填料或導電性粒子用時具有優勢,最佳為適用於導電性接著劑、導電性薄膜或導電性調距物。
導電性接著劑係區分為各向同性之導電性接著劑(ICA:Isotropic Conductive Adhesive)與各向異性之導電性接著劑(ACA:Anisotropic Conductive Adhesive)。又,依據黏合劑之形態可為糊料狀、薄膜狀、油墨狀之形態。各向同性之導電性接著劑為,黏合劑硬化時黏合劑會收縮,同時使長方向、寬方向及斜方向之填料相互接觸,藉
此使欲連結之導電物與填料接觸而得導電性。各向同性之導電性接著劑也可形成薄片。各向異性之導電性接著劑為,塊料係分散於黏合劑中而以所欲連結之導電物相互間挾持各向異性之導電性接著劑。其次將其長方向加壓,使長方向上欲連結之導電物之間的填料與欲連結之導電物接觸而得導電性。又,未加壓之部分係介有絕緣物之黏合劑而將填料群配置於寬方向,因未相互接觸故無法得到導電性。
導電性接著劑如,各向異性或各向同性之導電性糊料、各向異性或各向同性之導電性油墨等。導電性接著劑係由,使用遊星混合機或三座輥混合機般之混練機均勻混合由本實施形態之銀被覆粒子P1所形成之導電性粒子與絕緣性之黏合劑樹脂調製所得。導電性接著劑中,導電性粒子係均勻分散於絕緣性之黏合劑樹脂中。銀被覆粒子P1之含量無特別限定,可因應用途等而適當決定,但相對於黏合劑樹脂100質量份較佳為0.5~5質量份之範圍。
導電性接著劑中絕緣性之黏合劑樹脂無特別限定,例如熱塑性樹脂、硬化性樹脂組成物等之藉由熱或光而硬化之組成物等。熱塑性樹脂如,苯乙烯-丁二烯嵌段共聚物、丙烯酸酯樹脂、乙烯-乙酸乙烯樹脂等。硬化性樹脂組成物如,含有具有縮水甘油基之環氧系單體或低聚物,與異氟酸酯等之硬化劑的樹脂組成物。
導電性薄膜為,成形為薄膜狀之各向異性或各向同性之導電性薄膜。導電性薄膜係藉由,首先將由本實施形態之銀被覆粒子P1所形成之導電性粒子分散於絕緣性之黏合劑樹脂中製作樹脂組成物,其次將該樹脂組成物塗佈於PET等之支撐薄膜之表面所得。該樹脂組成物係由,使用遊星混合機或或三座輥混合機等之混練機均勻混合導電性粒子與絕緣性之黏合劑樹脂調製所得。導電性薄膜中,支撐體薄膜上導電性粒子係均勻分散於絕緣性之黏合劑樹脂中。導電性薄膜中絕緣性之黏合劑樹脂如,含有主成分用之環氧樹脂、苯氧樹脂等之熱硬化性樹脂的樹脂組成物。導電性薄膜中樹脂組成物中之銀被覆粒子P1之含量無特別限制,可因應用途等而適當決定,但相對於黏合劑樹脂100質量份較佳為0.5~10質量份之範圍。
導電性調距物為,液晶顯示裝置中以電氣上下連結挾持液晶物質的上下2枚基板之配線部分,且使基板間隙保持一定尺寸。導電性調距物係藉由,首先將由本實施形態之銀被覆粒子P1所形成之導電性粒子加入熱硬化性樹脂或紫外光硬化型接著劑等絕緣性之黏合劑樹脂後,使用遊星混合機或三座輥混合機等之混練機均勻混合導電性粒子與黏合劑樹脂,調製上述樹脂組成物後塗佈於上下2枚基板之配線部分之任何一方或雙方上,再貼合2枚基板所
得。銀被覆粒子P1之含量無特別限定,可因應用途等而適當決,但相對於黏合劑樹脂100質量份較佳為2~10質量份之範圍。
含有由本實施形態之銀被覆粒子P1所形成之導電性粒子的導電性接著劑、導電性薄膜或導電性調距物為,既使混練導電性粒子與絕緣性之黏合劑樹脂的混合物時施加高剪斷力,也不易使銀被覆層1發生龜裂或斷裂或由芯粒子2剝離銀被覆層1,可進一步提升其導電性。藉此例如本發明之銀被覆粒子P1係使用於各向異性之導電性接著劑時,可避免異向導電(寬方向)短路,而提升信賴性。
下面詳細說明本發明之實施例及比較例。
首先使用容量1dm3之量瓶,以水將氯化亞錫20g及濃度35%之鹽酸15cm3稀釋(女式)為1dm3,後保溫於30℃。藉由將作為母體之芯粒子用的平均粒徑10μm之球狀丙烯酸-苯乙烯共聚物樹脂50g加入該水溶液內,攪拌1小時後,濾取丙烯酸-苯乙烯共聚物樹脂再水洗之方式進行前處理。
其次藉由無電解電鍍於上述前處理後表面形成錫吸附層之丙烯酸-苯乙烯共聚物樹脂之表面上形成銀
被覆層。具體為,首先將作為錯化劑用之伸乙基二胺四乙酸鈉40g、作為pH調整劑用之氫氧化鈉20.0g、作為還原劑用之甲醛水(甲醛濃度37質量%)15ml加入水2dm3內,溶解調製含有錯化劑及還原劑之水溶液。其次將上述前述處理後之丙烯酸-苯乙烯共聚物樹脂浸漬於該水溶液內,調製漿液。
其次混合硝酸銀30g、25%氨水35ml、水50ml調製含有硝酸銀之水溶液,攪拌上述漿液的同時滴入該含有硝酸銀之水溶液。又,滴入氫氧化鈉使滴入含有硝酸銀之水溶液後之漿液的pH調整為12後,保持25℃之溫度的同時進行攪拌,而於樹脂表面上析出銀。其後進行洗淨及過濾,最後使用真空乾燥機以60℃之溫度乾燥,得銀被覆粒子先驅物。使用325mesh之不銹鋼平織所得之金屬網與振動篩由該銀被覆粒子先驅物捕集形成塊狀之粒子後,將捕集所得之銀被覆粒子先驅物舖滿於不銹鋼板上使厚度為1mm後,置於電氣馬弗爐內以30分鐘升溫至140℃,同溫度下保持4小時進行熱處理,燒結銀被覆層之銀結晶粒,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑3μm之球狀丙烯酸-苯乙烯共聚物樹脂,調整電鍍之銀質量。又,熱處理時之溫度為150℃,保持時間為3小時。除此以外同實施例1進
行,得相對於銀被覆粒子100質量%之銀量為65重量%之銀被覆粒子。以環氧樹脂固定該銀被覆粒子後切片,再以TEM(Transmission Electron Microscope)觀察。該銀被覆粒子之銀被覆層剖面之TEM像(倍率50萬倍)如圖1所示。圖1中銀被覆層1之內側為母體之芯粒子2,銀被覆層之外側為固定用之樹脂3。
母體之芯粒子係使用平均粒徑1μm之球狀丙烯酸-苯乙烯共聚物樹脂,調整電鍍之銀質量。又,熱處理時之溫度為120℃,保持時間為7小時。除此以外同實施例1相同,得相對於銀被覆粒子100質量%之銀量為90質量%之銀被覆粒子。
除了母體之芯粒子係使用平均粒徑20μm之球狀丙烯酸-苯乙烯共聚物樹脂,調整電鍍之銀質量外,同實施例1進行,得相對於銀被覆粒子100質量%之銀量為25質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑40μm之球狀丙烯酸-苯乙烯共聚物樹脂,調整電鍍之銀質量。又,熱處理時之溫度為160℃,保持時間為1.5小時。除此以外同實施例1
進行,得相對於銀被覆粒子100質量%之銀量為15質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂,調整電鍍之銀質量。又,熱處理時之溫度為130℃,保持時間為4小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為20質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂,調整電鍍銀質量。又,熱處理時之溫度為160℃,保持時間為6小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為80質量%之銀被覆粒子。
母體之芯粒子係使用同實施例5之丙烯酸-苯乙烯共聚物樹脂,調整電鍍之銀質量。除此以外同實施例5進行,得相對於銀被覆粒子100質量%銀量為5質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂。實施例1之大氣中之熱處理係以100℃進行。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂。實施例1之大氣中之熱處理係以200℃進行。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂。實施例1之大氣中之熱處理係進行0.5小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂。實施例1之大氣中之熱處理係進行10小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂。除了未進行實施例1之乾燥外,同實施例1得銀被覆粒子先驅物。於水中熱處理所得之銀被覆粒子先驅物。具體為,以10質量%般將該銀被覆粒子先驅物懸浮於離子交換水後,置於高壓釜中以150rpm之回轉速度攪拌該懸浮液的同時,150℃之溫度下保持3小時進行熱處理,燒結銀被覆層之銀結晶粒後,使用真空乾燥機以60℃之溫度乾燥過濾懸浮液所得之塊物。藉此得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑10μm之球狀苯酚樹脂,熱處理時之溫度為160℃,保持時間為1小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑10μm之球狀聚苯乙烯樹脂,熱處理時之溫度為120℃,保持時間為8小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑2μm之球狀聚矽氧樹
脂,調整電鍍之銀質量。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為80質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑10μm之棒狀經粉化之聚矽氧樹脂,調整電鍍之銀質量。又,熱處理時之溫度為130℃,保持時間為5小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為50質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑8μm之板狀氧化硼粉末,調整電鍍之銀質量。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為60質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑5μm之鱗片狀滑石粉末,調整電鍍之銀質量。又,熱處理時之溫度為150℃,保持時間為3小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為70質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑10μm之球狀聚矽氧橡膠粒子,調整電鍍之銀質量。又,熱處理時之溫度為245℃,保持時間為1小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂。同實施例1得銀被覆粒子先驅物。所得之銀被覆粒子先驅物不進行熱處理。藉此得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用同實施例2之丙烯酸-苯乙烯共聚物樹脂。同實施例2得銀被覆粒子先驅物。所得之銀被覆粒子先驅物不進行熱處理。藉此得相對於銀被覆粒子100質量%之銀量為65質量%之銀被覆粒子。同實施例2以環氧樹脂固定該銀被覆粒子後切片,再以TEM觀察。該銀被覆粒子P2之銀被覆層剖面之TEM像(倍率50萬倍)如圖2所示。圖2中銀被覆層11之內側為母體之芯粒子12,銀被覆層之外側為固定用樹脂13。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共
聚物樹脂。實施例1之大氣中之熱處理係進行0.25小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂。實施例1之大氣中之熱處理係進行11小時。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂。實施例1之大氣中之熱處理係以90℃進行。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用同實施例1之丙烯酸-苯乙烯共聚物樹脂。實施例1之大氣中之熱處理係以255℃進行。除此以外同實施例1進行,得相對於銀被覆粒子100質量%之銀量為45質量%之銀被覆粒子。
母體之芯粒子係使用平均粒徑3μm之鱗片狀滑石粉
末,調整電鍍之銀質量。除此以外同實施例1得銀被覆粒子先驅物。所得之銀被覆粒子先驅物不進行熱處理。藉此得相對於銀被覆粒子100質量%之銀量為78質量%之銀被覆粒子。
實施例1~19及比較例1~7之芯粒子之材質、平均粒徑、銀被覆粒子之銀量、製造銀被覆粒子時之熱處理環境、熱處理溫度及熱處理時間如表1所示。表1中「AS樹脂」各自為「丙烯酸-苯乙烯共聚物樹脂」。
各自以下述方法評估實施例1~20及比較例1~7所得
之銀被覆粒子中銀被覆層之平均膜厚、銀被覆層之銀結晶粒徑、施加剪斷應力前後之銀被覆層之外觀及壓縮20%時之施加剪斷應力前後的銀被覆粒子之電阻值。該些結果係如表2所示。
銀被覆層之平均膜厚係由,以平均膜厚為d、芯粒子之平均粒徑除以2所得之值為r、芯粒子之比重為dcore、銀之比重為dAg、銀被覆粒子中之銀質量與銀被覆粒子之質量之比為a,藉由下述式算出。
銀被覆層之銀結晶粒徑係由,將前述銀被覆粒子填入X線衍射裝置所附屬之試料托盤內以2 θ/θ=30~120deg之範圍照射X線,由所得之衍射線算出。該實施形態中,銀被覆層之銀結晶粒徑係使用PANalytical公司製之X線衍射裝置Empyrean,將所得之粉末狀銀被覆粒子填入該
裝置所附屬之試料托盤內以2 θ/θ=30~120deg之範圍照射X線,再由所得之衍射線使用解析軟體TOPAS(Bruker AXS公司製),以外形函數係使用FP之Pawley法解析,再由洛輪滋函數成分之半值幅算出。測定時係使用Cu管球,以40kV、40mA及特性X線(波長1.54Å)以分級間隔為0.025deg方式進行。藉由該Pawley法解析以求取銀被覆層之銀結晶粒徑。又,參考用之銀結晶粒徑之測定方法係使用謝勒式之方法。該方法為前述專利文獻2中測定銀結晶粒徑用之方法(參考專利文獻2之段落[0021])。該方法係以算出銀結晶之(111)面、(200)面、(220)面及(311)面中結晶粒徑之平均值作為結晶粒徑之值。又謝勒式為Dnk1=K λ/β cos θ(式中,Dnk1:結晶粒大小[m],λ:測定X線波長[m],K:定數=0.9,β:半值幅[rad],θ:衍射線之布雷格角[rad])。藉由本發明之測定法所得之測定值與參考用之使用謝勒式之方法求取的專利文獻2之請求項1所記載「銀結晶粒徑為18~24nm之範圍」,於藉由本發明之測定法求取時會為「銀結晶粒徑為26~34nm之範圍」。
藉由下述方法進行剪斷應力試驗。使用遊星混合機(新吉公司練太郎)使銀被覆粒子80質量份與乙二醇20質量份形成糊料狀混合物。以三座輥混合機(EXACT公司M-80E)重覆混練該糊料狀混合物10次後,將剪斷應力施加
於銀被覆粒子。此時三座輥之回轉速度為30rpm、55rpm及100rpm,輥間之間隔設定為銀被覆粒子之粒徑5倍之值。使用日立高科技股份公司製掃描型電子顯微鏡(型號:S-4300SE)觀察銀被覆粒子施加剪斷應力前後之銀被覆粒子之外觀進行評估。此時將銀被覆層發生龜裂、斷裂或由芯粒子剝離銀被覆層之銀被覆粒子為全體之5%以下之狀態視為外觀A、5~20%之狀態視為外觀B、20~100%之狀態視為外觀C。
以上述(3)所記載之方法對銀被覆粒子進行剪斷應力試驗。又,於剪斷應力試驗之前後進行銀被覆粒子之壓縮試驗。該壓縮試驗係以,使用微小壓縮試驗機(島侓製作所製,MCT-W200J)由上下方向壓縮1個銀被覆粒子之狀態進行。壓縮率於球狀粒子時為20%,於板狀粒子等長邊與短邊之長寬比為2以上之粒子時為5%。使用相同裝置藉由通電測定壓縮時之銀被覆粒子之電氣性電阻值。以上述條件各自測定10個銀被覆粒子,再以其電阻值之平均作為測定值。
由表2得知,實施適當熱處理而控制結晶粒徑之實施例1~2、實施例4~5、實施例13~18之銀被覆粒
子於施加剪斷應力前後之電鍍外觀及壓縮時之電阻值幾乎無變化,為適用於導電性接著劑及導電性調距物之用途的銀被覆粒子。又,銀被覆粒子中之銀量為上限值之實施例3中,增加銀量雖會提高成本,但同上述施加剪斷應力前後之電鍍外觀及壓縮時之電阻值幾乎無變化,為適用於接著劑及導電性調距物之用途的銀被覆粒子。
銀之結晶粒徑為下限值之實施例6及為上限值之實施例7中,施加剪斷應力前後之壓縮時之電阻值多少有變化,但包含外觀為良好之銀被覆粒子。
銀被覆粒子之銀量為下限值之實施例8中,初期電阻值稍微高些,但施加剪斷應力前後之變化小,包含外觀為良好之銀被覆粒子。
以較低溫度進行熱處理溫度之實施例9,及熱處理時間較短之實施例11中,因應處理可使結晶粒徑為較小之值。又,施加剪斷應力前後之壓縮時之電阻值會有某程度改變,但包括外觀為良好之銀被覆粒子。
熱處理溫度為較高溫之實施例10及實施例20、熱處理時間較長之實施例12中,結晶粒徑會大幅增加,但為外觀、電阻值均良好之銀被覆粒子。
芯粒子使用無機物之滑石的實施例19中,壓縮時之電阻值較高,但施加剪斷應力前後之其變化程度較小,包含外觀為良好之銀被覆粒子。
又,未實施熱處理之比較例1、2和7之銀被覆粒子,熱處理時間未達0.5小時之比較例3之銀被覆粒
子,及熱處理溫度未達100℃之比較例5之銀被覆粒子中,因其結晶粒徑低至35nm,故施加剪斷應力後銀會剝離,將有損外觀,且壓縮時之電阻值為較高之1000以上之值,故為不適用於導電性粒子之狀態。
熱處理時間超過10小時之比較例4之銀被覆粒子及熱處理溫度為250℃以上之比較例6之銀被覆粒子中,因熱處理時間太長會使結晶粒徑高至200nm,而過度燒結會因銀被覆層收縮而使銀被覆粒子變形,確認施加剪斷應力前後雙方會有部分銀剝離而有損外觀,且壓縮時之電阻值各自為較高之820Ω、1000Ω以上之值,故為不適用於導電性粒子之狀態。
由表示實施例2之銀被覆粒子的銀被覆層剖面之TEM像(倍率50萬倍)的圖1得知,藉由燒結銀被覆層中之銀以增加結晶粒徑,可使銀被覆層以無間隙方式被覆於芯粒子。結果施加剪斷力後銀被覆層也不會剝離,可保持平滑之被覆層。又,由表示比較例2之銀被覆粒子的銀被覆層剖面之TEM像(倍率50萬倍)的圖2得知,因銀被覆層中之銀結晶較小,故銀被覆層無法以無間隙方式被覆於芯粒子。結果施加剪斷應力時會因破壞粒界而使銀剝離。
本發明之銀被覆粒子適用為各向異性或各向同性之導電性接著劑、各向異性或各向同性之導電性薄膜
及導電性調距物之導電性填料或銀被覆粒子。
1‧‧‧銀被覆層
2‧‧‧芯粒子
3‧‧‧固定用樹脂
Claims (5)
- 一種銀被覆粒子,其為備有由樹脂粒子或無機粒子所形成之芯粒子,與形成於該芯粒子之表面上之銀被覆層的銀被覆粒子中,前述銀被覆層所含有之銀量相對於銀被覆粒子100質量份為5~90質量份,將前述銀被覆粒子填入X線衍射裝置所附屬之試料托盤內以2 θ/θ=30~120deg之範圍照射X線,再由所得之衍射線算出的前述銀之結晶粒徑為35~200nm之範圍。
- 一種銀被覆粒子之製造方法,其為包含將由樹脂粒子或無機粒子所形成之芯粒子加入錫化合物之水溶液而於前述芯粒子之表面上形成錫吸附層之步驟,與使用還原劑使形成於前述芯粒子之表面上之錫吸附層進行無電解銀電鍍而製作前述芯粒子之表面具有銀被覆層的銀被覆粒子先驅物之步驟,與水洗前述銀被覆粒子先驅物後乾燥再以大氣中100℃以上未達250℃之溫度或水洗後立刻以水中100℃以上未達250℃之溫度熱處理0.5~10小時而燒結構成前述銀被覆層之銀,使藉由X線衍射法測定之前述銀之結晶粒徑為35~200nm之範圍之步驟。
- 一種製造導電性接著劑之方法,其為藉由混合如請求項1之銀被覆粒子與黏合劑樹脂所得。
- 一種製造導電性薄膜之方法,其為藉由將混合如請求項1之銀被覆粒子與黏合劑樹脂所形成之樹脂組成物 塗佈於支撐薄膜表面所得。
- 一種製造導電性調距物之方法,其為藉由將混合如請求項1之銀被覆粒子與黏合劑樹脂所形成之樹脂組成物塗佈於2片基板中任何一方或雙方之表面後,貼合前述2片基板所得。
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GB201116240D0 (en) | 2011-09-20 | 2011-11-02 | Henkel Ag & Co Kgaa | Electrically conductive adhesives comprising silver-coated particles |
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CN107210090A (zh) | 2017-09-26 |
EP3252780A4 (en) | 2018-09-26 |
TWI662151B (zh) | 2019-06-11 |
KR20170108017A (ko) | 2017-09-26 |
KR102226646B1 (ko) | 2021-03-10 |
US10590540B2 (en) | 2020-03-17 |
EP3252780A1 (en) | 2017-12-06 |
EP3252780B1 (en) | 2020-03-04 |
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US20180016679A1 (en) | 2018-01-18 |
JP6665514B2 (ja) | 2020-03-13 |
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